23 results about "Phosphorus pentachloride" patented technology

This invention relates to a method for preparing high-purity phosphorus pentasulfide using a low-temperature liquid phase and its application, belonging to the technical field of key materials for lithium-sulfur batteries and solid-state batteries. It solves the technical problems of high reaction temperature and high energy consumption in existing phosphorus pentasulfide preparation processes. The method includes the following steps: Step 1: Select phosphorus pentachloride, dry it, and place the treated phosphorus pentachloride in an organic solvent to form a suspension or slurry system; Step 2: Place the suspension or slurry system in a closed reactor; Step 3: Introduce a sulfur source into the reactor to allow phosphorus pentachloride to undergo a sulfidation reaction with the sulfur source; Step 4: Raise the temperature to a set point and maintain a deep sulfidation reaction to generate phosphorus pentasulfide; Step 5: After the reaction, cool, separate the solid and liquid phases, and dry to obtain the solid product of phosphorus pentasulfide. This invention features mild reaction conditions, a simplified process flow, high safety, and recyclable solvents, making it suitable for continuous and large-scale production.

The utility model discloses a kind of even feeding devices for phosphorus pentachloride production, it is related to phosphorus pentachloride production technical field, including base, the top of base both ends is fixedly connected with U-shaped support seat, the top of base one end is fixedly connected with L-shaped support plate, both ends The top of U-shaped support seat is fixedly connected with heat-insulating jacket device, the inner side wall top of heat-insulating jacket device is fixedly connected with storage bin between, the bottom output end of storage bin is fixedly connected with electric valve, the other end of electric valve is fixedly connected with buffer tank, the base provided in the utility model, on the basis of realizing heat preservation protection to avoid affecting even feeding, increase inert gas protection to avoid causing metamorphosis simultaneously, to solve the temperature of the existing phosphorus pentachloride production feeding device is difficult to control due to lack of effective heat preservation structure, and lack of inert gas protection causes security and metamorphosis problem.

The utility model discloses phosphorus pentachloride anti-caking storage equipment which comprises supporting legs and a storage tank arranged on the supporting legs, the phosphorus pentachloride anti-caking storage equipment further comprises a heat dissipation assembly arranged in the storage tank, a storage cavity and a preparation cavity are sequentially arranged in the storage tank from top to bottom, the storage cavity and the preparation cavity are communicated through a discharging pipe, and the storage cavity is communicated with the preparation cavity. A first valve is arranged on the discharging pipe, the preparation cavity is communicated with the outside through a discharging pipe, a second valve is arranged on the discharging pipe, a flow dividing pipe, a first air inlet pipe, a first exhaust pipe, a second air inlet pipe and a second exhaust pipe are arranged on the storage tank, the first air inlet pipe is arranged on the storage tank and communicated with the storage cavity, and the second air outlet pipe is arranged on the storage tank and communicated with the storage cavity. A third valve is arranged on the first air inlet pipe, and the flow dividing pipe is arranged on the first air inlet pipe. The utility model relates to the technical field of phosphorus pentachloride storage, in particular to phosphorus pentachloride anti-blocking storage equipment which is not prone to being affected with damp, facilitates heat dissipation and is better in heat dissipation effect.

The utility model relates to the technical field of phosphorus pentachloride production devices, in particular to a phosphorus pentachloride production device which comprises a reaction box and a cover body covering the upper end of the reaction box, a stirring assembly is arranged on the cover body, and a filtering unit is arranged at the upper end of the cover body. The filtering unit comprises a shell and a Z-shaped plate, the shell is fixedly connected with the cover body, the Z-shaped plate is fixed with the shell through a fixing assembly, and a chlorine supply assembly is arranged on the lower side of the reaction box. Meanwhile, chlorine is continuously conveyed into the reaction box through the chlorine supply assembly and filtered through the filtering unit, a Z-shaped plate sealing structure is adopted, when activated carbon in a filtering frame is replaced, the lower side plate face of a Z-shaped plate can automatically seal the reaction box, chlorine leakage is effectively prevented, and the safety and operation convenience of the device are remarkably improved.

The invention relates to the technical field of organic synthesis, in particular to a preparation method of 2-chloro-6-trichloromethylpyridine. The method comprises the following steps: by taking 6-hydroxypyridine-2-carboxylic acid as a raw material, exposing an active group through acidification hydrolysis, then taking a composite solid-phase catalyst as a catalytic chlorinating agent, enabling the activated 6-hydroxypyridine-2-carboxylic acid to react with phosphorus pentachloride, carrying out primary chlorination on hydroxyl and carboxyl to obtain chlorine and acyl chloride, and continuously chlorinating acyl chloride to form trichloromethyl, by introducing the high-selectivity composite solid-phase catalyst, the problems of low yield and low selectivity in the existing preparation process of the 2-chloro-6-trichloromethylpyridine are solved, and meanwhile, the used catalyst is simple to recover.

The invention discloses tris (trimethylsilyl) phosphate and a preparation method thereof, and belongs to the field of chemical synthesis. The invention relates to a preparation method of tris (trimethylsilyl) phosphate, in particular to a preparation method of tris (trimethylsilyl) phosphate, which comprises the following steps: hexamethyldisiloxane and phosphorus pentafluoride are subjected to heating reaction under a stirring condition to obtain tris (trimethylsilyl) phosphate, and the molar ratio of hexamethyldisiloxane to phosphorus pentafluoride is (5-10): 1. Phosphorus pentachloride is replaced with phosphorus pentafluoride, and due to the fact that fluorine atoms are small in radius and large in electronegativity, phosphorus is high in electropositivity and small in steric hindrance, phosphorus pentafluoride can react with hexamethyldisiloxane more easily, a catalyst is not needed, the cost of tris (trimethylsilyl) phosphate can be greatly reduced, and the yield of tris (trimethylsilyl) phosphate is high.

The invention relates to the technical field of organic synthesis, in particular to 3-chloro-L-alanine hydrochloride and a preparation method thereof. The preparation method comprises the following steps: S1, continuously feeding a phosphorus pentachloride solution and a serine methyl ester hydrochloride solid into a dynamic tubular reactor for reaction, and carrying out solid-liquid separation, washing and drying on the reacted material to obtain 3-chloroserine methyl ester hydrochloride; and S2, mixing the 3-chloroserine methyl ester hydrochloride with hydrochloric acid, refluxing with boiling water, and drying to obtain the 3-chloro-L-alanine hydrochloride. According to the method, the reaction efficiency is greatly improved, meanwhile, the safety is good, the prepared product is high in yield and purity, and the method is suitable for industrial production.

The invention provides a treatment method of tail gas containing phosphorus pentafluoride and a preparation method and device of lithium hexafluorophosphate. The treatment method of the tail gas containing phosphorus pentafluoride comprises the following steps: 1) carrying out first absorption treatment on the tail gas containing phosphorus pentafluoride by adopting a first absorption liquid containing lithium fluoride to obtain a first lithium hexafluorophosphate solution and a first mixed gas containing hydrogen fluoride; 2) carrying out first reaction on phosphorus pentachloride and the first mixed gas to obtain second mixed gas containing phosphorus pentafluoride; and 3) carrying out second absorption treatment on the second mixed gas by using a second absorption liquid containing lithium fluoride to obtain a second lithium hexafluorophosphate solution and a third mixed gas containing hydrogen fluoride and hydrogen chloride. According to the treatment method of the tail gas containing phosphorus pentafluoride, provided by the invention, the content of phosphorus pentafluoride in the tail gas can be reduced, and the resource utilization rate is improved.

The application relates to the technical field of phosphorus pentafluoride preparation, and provides a phosphorus pentafluoride gas generator, which comprises a generator cylinder body and a filtering structure, the generator cylinder body is internally provided with a reaction cavity, the generator cylinder body comprises an upper cylinder body and a lower cylinder body, the upper cylinder body is provided with a first feeding port for feeding phosphorus pentachloride solids into the reaction cavity, and the lower cylinder body is provided with a second feeding port for feeding hydrogen fluoride liquid into the reaction cavity; the filtering structure is arranged between the reaction cavity and the second feeding port, and is used for permeating the hydrogen fluoride liquid and blocking the phosphorus pentachloride solids. The phosphorus pentafluoride gas generator provided by the application can make the hydrogen fluoride liquid and the phosphorus pentachloride solids fully contact in the reaction cavity by arranging the filtering structure for permeating the hydrogen fluoride liquid and blocking the phosphorus pentachloride solids, so that the reaction rate is improved, and the preparation efficiency of phosphorus pentafluoride gas is improved.

The utility model discloses phosphorus pentachloride feeding reaction equipment which comprises a reaction kettle, a feeding assembly is mounted at the top of the reaction kettle, the feeding assembly comprises a mounting cover fixedly connected with the outer wall of the top of the reaction kettle, the mounting cover is communicated with the inner space of the reaction kettle, two connecting holes are formed in the middle of the mounting cover, and the connecting holes are communicated with the mounting cover. The interiors of the two connecting holes are rotationally connected with the same feeding ring through bearings, the circumferential outer wall of the feeding ring is attached to the circumferential inner wall of the mounting cover, a vertically-arranged storage cavity is formed in the middle of the feeding ring, a piston is slidably inserted into the storage cavity, and the inner walls of the two sides of the storage cavity are each provided with two limiting strips; according to the phosphorus pentachloride feeding device, through the arrangement of the feeding assembly, it is guaranteed that phosphorus pentachloride can be smoothly fed into the reaction kettle, meanwhile, poisonous gas generated by reaction cannot be mixed into the storage cavity, and the safety of the device can be improved.

The preparation method comprises the following steps: dissolving phosphorus pentachloride in an n-hexane solvent, and preparing a phosphorus pentachloride solution with the concentration of 20 to 50 mmol / L; immersing the original chinlon in a phosphorus pentachloride solution for activation reaction to obtain activated chinlon; taking out the activated chinlon and removing the residual phosphorus pentachloride solution on the surface; the cleaned chinlon is immersed in a hyperbranched polylysine solution with the concentration of 15-30 wt% for a grafting reaction, and grafted chinlon is obtained; taking out the grafted chinlon, and removing residual substances on the surface of the grafted chinlon; and drying the washed chinlon to obtain the modified chinlon. According to the modified chinlon, a phosphorus pentachloride activation-hyperbranched polylysine grafting two-step method is adopted, the mechanical property of the chinlon is effectively protected while the efficient antibacterial and deodorizing functions are achieved, the antibacterial and deodorizing effect has good durability, and therefore the problems that in the prior art, modified chinlon is poor in antibacterial durability, large in fiber damage and the like are solved.

The application relates to a method for preparing high-purity phosphorus pentasulfide in a low-temperature liquid phase and application thereof, and belongs to the technical field of key materials for lithium-sulfur batteries and solid-state batteries. The method solves the technical problems of high reaction temperature and large energy consumption in the existing preparation process of phosphorus pentasulfide. The method comprises the following steps: step 1, selecting phosphorus pentachloride, drying the phosphorus pentachloride, and placing the treated phosphorus pentachloride in an organic solvent to form a suspension phase or a slurry system; step 2, placing the suspension phase or the slurry system in a closed reactor; step 3, introducing a sulfur source into the reactor to make the phosphorus pentachloride and the sulfur source undergo a sulfuration reaction; step 4, keeping the deep sulfuration reaction after being heated to a set temperature to generate phosphorus pentasulfide; and step 5, cooling, solid-liquid separation and drying after the reaction to obtain a phosphorus pentasulfide solid product. The application has the advantages of mild reaction conditions, simplified process flow, high safety, recyclable solvent and suitability for continuous and large-scale production.

The invention relates to the technical field of organic synthesis, and particularly discloses a preparation process of linear phenoxy phosphazene. The method comprises the following steps: adding ammonium chloride and phosphorus pentachloride into a solvent, and heating to 140-180 DEG C under the catalysis of an acidic ionic liquid to synthesize linear chlorophosphazene; after the reaction is completed, filtering the system while the system is hot, and pulping by adopting n-heptane to obtain linear chlorophosphazene; sequentially adding phenol and alkali into the solution, heating to 70 DEG C under the protection of nitrogen, and carrying out nucleophilic substitution reaction; and after the reaction is finished, concentrating the solvent, removing residual excessive phenol in the system through alkali washing, and washing with water until the system is neutral to finally obtain a white solid product, namely the target product linear phenoxy phosphazene. According to the process, the acidic ionic liquid is introduced as a synergistic catalyst, so that the temperature required by the ring-opening reaction of the cyclic phosphazene is remarkably reduced, the process safety is improved, the production energy consumption is also greatly reduced, and the process is an energy-saving, environment-friendly and efficient linear phenoxy phosphazene synthesis path.

The application relates to the technical field of reaction kettle temperature control, in particular to a reaction kettle temperature stable control system and method for phosphorus pentachloride production, which comprises the following steps: collecting the chlorine consumption, the temperature in the kettle and the circulating water flow in the phosphorus pentachloride production process in real time; analyzing the correlation between the chlorine consumption and the circulating water flow in each sampling period to determine a trend reverse coefficient, and analyzing the trend change amplitude of the chlorine consumption and the circulating water flow and the correlation with the temperature to determine a trend amplitude influence coefficient; fusing the trend reverse coefficient and the trend amplitude influence coefficient to obtain a response adjustment coefficient, according to which the proportional parameter of a PID controller is dynamically adjusted, and the reaction kettle temperature in the next sampling period is controlled by using the adjusted PID controller. The application solves the problem that the traditional PID parameter fixation cannot adapt to temperature lag fluctuation, and improves the stability of the reaction kettle temperature control in the phosphorus pentachloride production process.

The present invention provides a mepivacaine preparation method, which comprises that in an organic solvent, 1-methylpiperidine-2-formic acid and 2, 6-dimethylaniline are subjected to a condensation reaction in the presence of a condensing agent to obtain mepivacaine, and the condensing agent is selected from one or more of phosphorus oxychloride, phosphorus trichloride and phosphorus pentachloride. The condensing agent used for preparing mepivacaine is one or more of phosphorus oxychloride, phosphorus trichloride and phosphorus pentachloride, toxic substances such as phosgene and the like are not generated, the safety is high, the cost is low, and the preparation method is suitable for industrial popularization.

This invention relates to a method for preparing compound (I) or a pharmaceutically acceptable salt or solvate thereof. In particular, such a method comprises the dehydration cyclization of a 1,2-diacylhydrazine intermediate to form the corresponding 1,3,4-oxadiazole, wherein the dehydration cyclizing agent may be N,N-dimethylaminosulfonyl chloride, N-(triethylammonium sulfonyl)carbamate, phosphorus trichloride, or phosphorus pentachloride, resulting in increased product yield and purity compared to known methods. Compound (I) and pharmaceutical compositions thereof can be used as respiratory syncytial virus (RSV) inhibitors.

The invention discloses an efficient and environment-friendly synthesis method for phosphonitrilic chloride, which comprises the following steps: under the action of a composite catalyst and the protection of nitrogen, reacting phosphorus pentachloride PCl5 with ammonium chloride NH4Cl in a solvent, and after the reaction is finished, carrying out post-treatment to obtain phosphonitrilic chloride, the main effective component of the composite catalyst is nicotinic acid or nicotinoyl derivatives, the nicotinic acid derivatives are at least one of nicotinic acid or ammonium nicotinate and salts thereof, and the nicotinoyl derivatives are at least one of nicotinamide and salts thereof; the secondary effective component of the composite catalyst is Lewis acid. According to the method, nicotinamide is used as a novel efficient catalyst for chemical reaction, a brand new application of nicotinamide is achieved, when nicotinamide is used for replacing pyridine as a catalyst to be applied to a reaction for synthesizing hexachlorocyclotriphosphazene by taking phosphorus pentachloride and ammonium chloride as raw materials, the reaction time can be shortened, the reaction yield is obviously increased, and the method is suitable for industrial production. And a good technical effect is achieved.

The invention discloses a preparation method of moisture-absorbing and quick-drying chinlon. The preparation method comprises the following steps: preparing a phosphorus pentachloride solution with the concentration of 20-50mmol / L; preparing a polyethyleneimine solution with the concentration of 2 to 10 weight percent; immersing the original chinlon in a phosphorus pentachloride solution for activation reaction to obtain activated chinlon; the activated chinlon is immersed in a polyethyleneimine solution for a grafting reaction, and grafted chinlon is obtained; the grafted chinlon is taken out and dried, and the modified chinlon is obtained. A hydrophilic polymer network is formed on the modified chinlon treated through the steps, and rapid moisture absorption, efficient conduction and rapid evaporation of moisture can be achieved through the hydrophilic polymer network, so that the moisture absorption and quick drying effects are achieved, and the requirements of sports suits, summer commuting suits, underwear and other easy-to-sweat scenes are met; the problems of stickiness, stuffiness and the like caused by sweat retention can be avoided.

The embodiment of the invention provides a regeneration method of trimethylchlorosilane. Comprising the following steps: carrying out chlorination reaction on hexamethyldisiloxane and phosphorus pentachloride to obtain trimethylchlorosilane and phosphorus oxychloride. According to the method, phosphorus pentachloride is used for replacing a highly toxic or highly corrosive reagent, hexamethyldisiloxane is safely and efficiently converted into trimethylchlorosilane under a mild condition, a high-value byproduct phosphorus oxychloride is synchronously recovered, and the method has the advantages of environmental protection and economy.

The application provides a lithium hexafluorophosphate concentrated solution and a preparation method and application thereof. The preparation method comprises the following steps: reacting lithium halide with phosphorus pentachloride in a solvent, then reacting with hydrogen fluoride to generate a lithium hexafluorophosphate solution, and then sequentially performing degassing, filtration, concentration, dilution and resin deacidification to obtain the lithium hexafluorophosphate concentrated solution. The preparation method is a continuous reaction scheme, can inhibit the risk of using hydrogen fluoride, and can improve the yield. Impurities are removed by degassing, filtration, concentration, dilution and deacidification resin, and further, byproduct can be collected to obtain high-purity hydrogen chloride for export and high-purity hydrogen fluoride for recycling. The preparation method has the characteristics of low equipment investment, simple operation, low cost, complete recycling of byproducts and the like, and is more suitable for industrial large-scale production. The lithium hexafluorophosphate concentrated solution product can be used as an electrolyte salt for lithium battery electrolyte, and has the same or higher battery performance as common lithium hexafluorophosphate crystals.

The utility model discloses anti-caking phosphorus pentachloride storage equipment, which relates to the field of phosphorus pentachloride and comprises a main storage box, bottom isolation pads are symmetrically and fixedly connected to the bottom surface of the main storage box in a threaded manner, a sealing cover plate is fastened to an opening in the side edge of the main storage box, and fixed screw discs are symmetrically inserted into the side edge of the sealing cover plate. A top clamping groove is horizontally formed in the top face of the main storage box, a supporting cover plate is horizontally connected to the inner side edge of the top clamping groove in a clamped mode, a control panel is fixedly connected to one side edge of the main storage box in a clamped mode, an overturning motor is fixedly arranged on one side edge of the main storage box, and a sealing inner groove is formed in the inner side edge of an opening of the main storage box. And fixing screw holes are symmetrically formed in the inner side edge of an opening of the main storage box, a rotating column body is horizontally arranged on the inner side edge of the main storage box, a sealing isolation structure is adopted, so that storage is safer and more reliable, and the situation of material caking is effectively prevented under the double structures of the rotating structure and dehumidification.

This invention discloses a method for preparing sodium difluorophosphate, comprising the following steps: reacting phosphorus pentachloride, phosphorus pentoxide, and sodium hydrogen fluoride as raw materials in an organic solvent; after the reaction, purging with inert gas, filtering, concentrating and crystallizing, washing, and drying to obtain sodium difluorophosphate. This method features low raw material cost, simple process, rapid reaction, few by-products, no water introduction, high product purity, and is environmentally friendly.